反应详情

To a cold solution of triphenylphosphine (1.8 g) in dry THF (90 mL) was added dropwise DEAD 40% in toluene (3.15 mL). Then was added successively phthalimide (1.01 g) and a solution of (3-benzyl-7,7-difluoro-3-azabicyclo[3.3.0]oct-2-yl)-methanol (WO03/062265) (1.83 g) in dry THF (10 mL). The reaction mixture was stirred at RT overnight, diluted with EA, washed with water. The organic phase was washed with sat. NaHCO3 solution, dried (MgSO4), filtered and concentrated to yield a crude oil. FC (n-heptane/EA: 7/3 to 1/1) gave 1.73 g (64%) of the title compound as a white solid. LC-MS: tR=0.87 min; [M+H]+=397.47.

1. washwashed with water
2. washThe organic phase was washed with sat. NaHCO3 solution
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customto yield a crude oil